CN107064363B - A method of flash distillation gas chromatography evaluates kadsura longepedunculata quality in commercially available Chinese patent drug - Google Patents
A method of flash distillation gas chromatography evaluates kadsura longepedunculata quality in commercially available Chinese patent drug Download PDFInfo
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Abstract
A method of flash distillation gas chromatography evaluates kadsura longepedunculata quality in commercially available Chinese patent drug, the method are as follows: (1) the powdered or liquid Chinese patent drug sample containing kadsura longepedunculata is fitted into cracker, cracker is placed at gas chromatograph injection port, the sample introduction when cracker temperature reaches certain temperature, it is detected with gas chromatograph, obtain gas chromatogram, qualitative analysis is carried out using the lignans in standard substance retention time centering analysing pharmaceutical samples, determines anwulignan in gas chromatogram, schizandrin A and the corresponding peak position of Schisantherin C；(2) then pass through schizandrin A and the Schisantherin C progress quantitative analysis in external standard method centering analysing pharmaceutical samples using Flash evaporation gas chromatography method, if quantitative result is shown, the relative amount of schizandrin A and Schisantherin C is fallen within the scope of 1.50-2.0 in Chinese patent drug sample, then contained kadsura longepedunculata quality is preferable in Chinese patent drug sample, otherwise second-rate.The present invention has the characteristics that simple and environmentally-friendly, efficient.
Description
(1) technical field
The present invention relates to a kind of methods for evaluating kadsura longepedunculata quality in commercially available Chinese patent drug.
(2) background technique
Kadsura longepedunculata is herbaceous plant Central China five tastes of growing nonparasitically upon another plant Schisandra chinensis chain timbers orchid family (Magnoliacae) Schizandra many years
The dry mature fruit of sub (Schisandraesphenanthera Rehd.et Wils.) mainly originates in Shaanxi, Sichuan and mountain
The middle parts such as west.Kadsura longepedunculata mainly contains a variety of chemical components such as lignanoid, volatile oil, Thick many candies and fatty acid, medicinal
The effect of value is very high, and traditional medicine thinks that it promotes the production of body fluid with astringing lung-QI, kidney tonifying nourishing heart, astringency inducing.It is generally believed that kadsura longepedunculata
Bioactivity mainly from lignanoid, especially using cyclohexyl biphenyl octene as the lignanoid of parent nucleus.Due to its very high medicinal valence
Value, therefore kadsura longepedunculata is used in various Chinese patent drugs, has the sum based on kadsura longepedunculata supplemented by kadsura longepedunculata.
For kadsura longepedunculata raw medicinal herbs, the Pharmacopoeia of the People's Republic of China (2015 editions) regulations, anwulignan
(anwulignan), one kind of lignans is to judge that the medicinal material is the index of kadsura longepedunculata；Schisantherin C
(schisantherin A), another lignans are the standards for judging kadsura longepedunculata quality, when dry south five
The content of Schisantherin C is more than 0.2% in taste medicinal material, then the kadsura longepedunculata quality meets States Pharmacopoeia specifications.But for containing south
The Chinese patent drug of Schisandra chinensis can be judged whether with anwulignan using can not obtain five but since kadsura longepedunculata usage amount is unknown
Relative quantity of the taste ester first relative to kadsura longepedunculata medicinal material also just can not judge kadsura longepedunculata in Chinese patent drug with the standard of pharmacopeia
Quality.Therefore need to find a new index to judge the quality of kadsura longepedunculata used in Chinese patent drug.
Lignanoid's detection method in Chinese patent drug of the existing literature to kadsura longepedunculata raw medicinal herbs and containing kadsura longepedunculata, often
Method has thin-layered chromatography, liquid chromatography, gas chromatography etc., but needs soak extraction, ultrasonic extraction, microwave-assisted
The cumbersome pretreatment modes such as extraction, and there is no literature reported on the quality evaluation sides of kadsura longepedunculata in the Chinese patent drug containing kadsura longepedunculata
Method.Therefore, the present invention searches out the finger for judging kadsura longepedunculata quality by lignanoid's content in measurement kadsura longepedunculata raw medicinal herbs
The index, is used for the judgement of kadsura longepedunculata quality in Chinese patent drug by mark.
(3) summary of the invention
It is an object of the present invention to provide a kind of methods that flash distillation gas chromatography evaluates kadsura longepedunculata quality in commercially available Chinese patent drug.
For achieving the above object, the technical solution adopted by the present invention is that:
A method of flash distillation gas chromatography evaluates kadsura longepedunculata quality, the method in commercially available Chinese patent drug are as follows:
(1) the powdered or liquid Chinese patent drug sample containing kadsura longepedunculata is fitted into cracker, cracker is placed in
At gas chromatograph injection port, the sample introduction when cracker temperature reaches certain temperature is detected with gas chromatograph, obtains gas phase color
Spectrogram carries out qualitative analysis using the lignans in standard substance retention time centering analysing pharmaceutical samples, determines gas-chromatography
Anwulignan, schizandrin A and the corresponding peak position of Schisantherin C in figure；If can determine that containing anwulignan, in this at
Contain kadsura longepedunculata in medicine sample；
(2) then pass through the schizandrin A and the five tastes in external standard method centering analysing pharmaceutical samples using Flash evaporation gas chromatography method
Sub- ester first carries out quantitative analysis, if quantitative result is shown, schizandrin A and the opposite of Schisantherin C contain in Chinese patent drug sample
Amount (P2/P10) is fallen within the scope of 1.50-2.0, then contained kadsura longepedunculata quality is preferable in Chinese patent drug sample, otherwise second-rate.
In the present invention, in order to ensure the uniformity and representativeness of sample, the powdered Chinese patent drug sample containing kadsura longepedunculata
Partial size is preferably 80~120 meshes.If the commercially available solid Chinese patent drug containing kadsura longepedunculata does not exist with powdery form, need
Comminution pretreatment is carried out to it, such as it is ground, 80~120 meshes is crossed, powdered samples is made.
In the present invention, qualitative and quantitative analysis condition is preferred are as follows:
The GC conditions are as follows: chromatographic column is low-pole column, UA-5 metal capillary column (30m × 0.25mmi.d.
× 0.25 μm of film thickness, 5% methyl polysiloxane, Japan), column temperature rise program is 50 DEG C of initial temperature, with 5~10 DEG C/min rate liter
300 DEG C are raised to 200 DEG C, then with 3~5 DEG C/min rate, then in 300 DEG C of 5~15min of holding；Injector temperature be 280~
320 DEG C, detector temperature is 280~320 DEG C, 30~50:1 of split ratio；Carrier gas is nitrogen or helium, flow velocity 1.0mL/min；
Cracker condition: cracking furnace temperature: 300-350 DEG C；Cracker with 300~350 DEG C of gas chromatograph interface temperature.
The further preferred GC conditions are as follows: column temperature rise program is 50 DEG C of initial temperature, with 10 DEG C/min rate liter
300 DEG C are raised to 200 DEG C, then with 5 DEG C/min rate, then in 300 DEG C of holding 10min；Injector temperature is 300 DEG C, detection
Device temperature is 300 DEG C.
It, can be according to each wood in the gas-chromatography spectrogram centering analysing pharmaceutical samples of kadsura longepedunculata raw medicinal herbs in step (1) of the present invention
The progress of rouge element ingredient is qualitative, and lignans are concentrated mainly between 25-45min.In addition, lignans is qualitative, may be used also
Using interpretation of mass spectra, Mass Spectrometry Conditions are preferred are as follows: electron impact ion source, 230~250 DEG C of ion source temperature, and transmission line temperature 250
~300 DEG C, ionizing energy 70eV, 50~650m/z of ion scan range.
In step (2) of the present invention, by external standard method in lignans schizandrin A and Schisantherin C carry out
Quantitative analysis is the methanol solution that the standard items of schizandrin A and Schisantherin C are made into 20-10000mg/L first, so
It is measured under the conditions of gas-chromatography same as Chinese patent drug sample and cracker afterwards, and standard song is made in test result
The content of schizandrin A and Schisantherin C in Chinese patent drug sample is calculated according to standard curve for line.
Compared with prior art, beneficial effect of the present invention is mainly reflected in: the present invention is commented with flash distillation gas chromatography-mass spectrography
On the one hand kadsura longepedunculata quality in the commercially available Chinese patent drug of valence flashes gas-chromatography using solid and (is directed to raw medicinal herbs and ball, capsule etc.
Dosage form Chinese patent drug) or liquid (being directed to soft capsule dosage form Chinese patent drug) sample direct injected, it is not necessarily to complex extraction process, it is solvent-free to make
With, therefore easy to operate, environmental protection；On the other hand qualitative and quantitative analysis is carried out to kadsura longepedunculata by flash chromatography-mass spectrometry method,
Experimental period can effectively be saved, simplify experimental procedure；Therefore, evaluation quality method of the invention has simple and environmentally-friendly, efficient
The characteristics of, which can be generalized to kadsura longepedunculata Quality estimation field, have to kadsura longepedunculata quality evaluation very deep
Remote meaning.
(4) Detailed description of the invention
Fig. 1 is the flash distillation gas chromatogram that Shaanxi produces kadsura longepedunculata (S1) and 8 lignanoid's standard items；
Fig. 2 is from 6 provinces Flash evaporation gas chromatography figure of totally 14 kadsura longepedunculata samples at 300 DEG C；
Fig. 3 is the flash distillation gas chromatogram of 6 kinds of commercially available Chinese patent drugs based on kadsura longepedunculata；
Fig. 4 is the Flash evaporation gas chromatography figure of 7 kinds of commercially available Chinese patent drugs supplemented by kadsura longepedunculata.
(5) specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited in
This:
Lignanoid's qualitative analysis in 1 kadsura longepedunculata raw medicinal herbs of embodiment
(1) instrument and reagent
The Gc/ms Analyser (GC-MS) of U.S. ThermoFinnigan Trace DSQ；The U.S.
ThermoFinnigan Trace GC Ultra gas chromatograph is matched hydrogen flame detector (FID)；Japanese Frontier PY-
3030D double click type longitudinal type micro furnace cracker.
Work as real estate Schisandra chinensis from Shaanxi, Sichuan, Shanxi, pharmacy's purchase, reject the sundries such as macroscopic branch, sawdust,
It is dried 5 hours in 60 DEG C, takes out quickly ground 120 mesh, Chinese Magnolivine Fruit is made, it is spare.Sample list is shown in Table 1.
Table 1: kadsura longepedunculata raw medicinal herbs sample list
(2) experimental method
It accurately weighs Shaanxi and produces kadsura longepedunculata (S1) powder 0.3mg loading specimen cup, after being fixed on sample feeding rod, be packed into installation
Cracker above GC injection port, sample is in room temperature at this time.After cracker temperature reaches suitable temperature, press sample introduction by
Button, specimen cup fall into the furnace heart, and volatile component transient evaporation brings GC injection port by carrier gas, carries out gas chromatographic analysis.
U.S.'s ThermoFinnigan Trace GC Ultra gas chromatograph (UA-5 metal capillary column, 30m ×
0.25mmi.d. × 0.25 μm, 5% methyl polysiloxane of film thickness, Japan), Japanese Frontier PY-3040D double click type longitudinal type
Micro furnace cracker.
Flash gas phase condition: UA-5 metal capillary column (30m × 0.25mmi.d. × 0.25 μm, 5% methyl polysilicon of film thickness
Oxygen alkane, Japan) temperature program: 50 DEG C of initial temperature, 200 DEG C are raised to 10 DEG C/min rate, then be raised to 300 DEG C with 5 DEG C/min rate,
Keep 10min；Injector temperature is 300 DEG C, and detector temperature is 300 DEG C, split ratio 30:1；Carrier gas nitrogen or helium, flow velocity
1.0mL/min.Cracker condition: cracking furnace temperature: 300 DEG C；Cracker with 300 DEG C of gas chromatograph interface temperature.
Mass Spectrometry Conditions are as follows: electron impact ion source, 230 DEG C of ion source temperature, 300 DEG C of transmission line temperature, ionizing energy
70eV, 40~550m/z of ion scan range.
(3) results and discussion
Lignanoid is kadsura longepedunculata main active, it is therefore desirable to carry out qualitative analysis to lignanoid in kadsura longepedunculata.
Fig. 1 is the Flash evaporation gas chromatography/mass spectrum total ion current figure and 8 lignanoid's standard items of kadsura longepedunculata raw medicinal herbs sample (S1)
Total ion current figure.It can be seen that peak of the retention time within the scope of 25-45min is lignanoid.12 wooden rouge are observed altogether
Element.Wherein 8 lignans, anwulignan (1), schizandrin A (2), deoxyschizandrin (3), schizandrin (4), five
Taste phenol (5), wuweizi alcohol B (6), wuweizi ester B (7) and Schisantherin C (10), when being by reservation with standard items
Between and mass spectrogram be compared to qualitatively.In addition, the mass spectrogram and No. 7 peaks at No. 8 peaks are identical, the mass spectrogram and 10 at No. 11 peaks
Number peak is identical, is respectively schisantherin C and Gomisin G according to Literature Consult.No. 10 peaks and No. 12 peak molecular ion peaks are identical,
But partial piece ion is not identical.According to the deduction and Literature Consult to its possible dissociation pathways, is distinguished and qualitative be
Benzoyl Gomisin O and schisantherin D.It the results are shown in Table 2.
Table 2: the qualitative results of lignanoid in kadsura longepedunculata raw medicinal herbs
The investigation of 2 reproducibility of embodiment
U.S. Thermo Trace GC ultra gas chromatograph (UA-5 metal capillary column, 30m × 0.25mmi.d.
× 0.25 μm, 5% methyl polysiloxane of film thickness, Japan), Japanese Frontier PY-3030D double click type longitudinal type micro furnace cracking
Device.
Gas phase condition: temperature program: 50 DEG C of initial temperature, 200 DEG C are raised to 10 DEG C/min rate, then with 10 DEG C/min rate liter
To 300 DEG C, 10min is kept；Injector temperature is 300 DEG C, and detector temperature is 300 DEG C, split ratio 30:1；Carrier gas nitrogen or helium
Gas, flow velocity 1.0mL/min.
Cracker condition: cracking furnace temperature: 300 DEG C；Cracker with 300 DEG C of gas chromatograph interface temperature.
The Shaanxi for accurately weighing 3 parts of 1 method of embodiment preparations respectively produces kadsura longepedunculata powder 0.3mg and is packed into specimen cup, Gu
After sample feeding rod, it is packed into the cracker being mounted on above GC injection port, sample is in room temperature at this time.Reach to cracker temperature
At 300 DEG C, sample introduction button is pressed, specimen cup falls into the furnace heart, and volatile component transient evaporation brings GC injection port by carrier gas, into
Row GC analysis.
The reproducibility (being indicated with relative standard deviation (RSD)) of the absolute peak area in computer chromatography peak.The results show that peak face
Long-pending RSD≤5.46% illustrates that flash distillation 0.3mg, 120 mesh Chinese Magnolivine Fruit samples can guarantee that experimental result obtains at 300 DEG C
Good reproducibility.
Lignanoid's quantitative analysis in 3 kadsura longepedunculata raw medicinal herbs of embodiment
The gas chromatograph Japan Frontier PY-2020iD double click type longitudinal type of U.S. ThermoFinnigan Trace
Micro furnace cracker.
Gas phase condition are as follows: chromatographic column is UA-5 metal capillary column (30m × 0.25mmi.d. × 0.25 μm, 5% first of film thickness
Based polysiloxane, Japan) column temperature rise program is 50 DEG C of initial temperature, 200 DEG C are raised to 10 DEG C/min rate, then with 10 DEG C/min speed
Rate is raised to 300 DEG C, keeps 10min；Injector temperature is 300 DEG C, and detector temperature is 300 DEG C, split ratio 30:1；Carrier gas is nitrogen
Gas or helium, flow velocity 1.0mL/min.
Cracker condition: cracking furnace temperature: 300 DEG C；Cracker with 300 DEG C of gas chromatograph interface temperature.
The standard items of 8 lignanoids are made into the methanol solution (mixed mark) of 20-10000mg/L, draw 1 microlitre of solution injection
In specimen cup, after being fixed on sample feeding rod after its solvent volatilizes, it is packed into the cracker being mounted on above GC injection port, at this time sample
In room temperature.When cracker temperature reaches 300 DEG C, sample introduction button is pressed, specimen cup falls into the furnace heart, mixes mark solution moment gas
Change, GC injection port is brought by carrier gas and carries out a point analysis of variance.
The parameters such as the linear of this method, detection limit and quantitative limit are investigated, the results are shown in Table 3.It can be seen that, pacify five from table 3
Rouge element is in 50-10000mg/L, other 7 lignanoids are linear good within the scope of 20-10000mg/L, and r is greater than 0.99.8 wood
Rouge element detection limit is between 1.52-6.09mg/L, and quantitative limit is between 5.04-20.3mg/L.And 100mg/L and 1000mg/L are dense
Lower RSD is spent less than 5.21%, therefore, it is considered that this method accuracy is good, can be used to measure lignanoid.
The linear of 3:8 lignanoid of table, detection limit and quantitative limit result
Lignans in 6 provinces totally 14 kadsura longepedunculata samples are measured.No. 8 peaks use No. 7
The linear equation at peak is quantified, and 9,11 and No. 12 peaks are quantified using the linear equation at No. 10 peaks.
Fig. 2 is the Flash evaporation gas chromatography figure of 14 kadsura longepedunculata raw medicinal herbs.Table 4 is the quantitative result of 12 lignanoids.From
It in figure and can be seen that in 14 samples in table and all contain anwulignan (No. 1 peak), it can be determined that 14 samples are all south five
Taste.The Schisantherin C that Schisantherin C (No. 10 peaks) meets States Pharmacopoeia specifications in S1-9 sample is not less than the content of 2mg/g,
Therefore, it is considered that this nine kadsura longepedunculata raw medicinal herbs quality are preferable；The content of Schisantherin C is below 2mg/g in S10-14 sample,
Therefore, it is considered that its is second-rate.Anwulignan (No. 1 peak), schizandrin A (No. 2 peaks) and Schisantherin C (10 in S1-9 sample
Number peak) content highest.
The content (mg/g) of 12 lignanoids in 4:14 kadsura longepedunculata sample of table
aN.D.: expression is not detected
bTr: it indicates to be lower than quantitative limit
c: the ratio between the content at No. 2 peaks and No. 10 peaks
For Chinese patent drug, since the kadsura longepedunculata quality wherein contained is unknown, this mark of 2mg/g cannot be passed through
Standard judges the quality of wherein kadsura longepedunculata.Due to schizandrin A content in the preferable sample of quality content highest, because
This attempts that the relative amount (P2/P10) of schizandrin A and Schisantherin C is used to be judged, the results are shown in Table 4.From table 4
As can be seen that in the preferable kadsura longepedunculata raw medicinal herbs of quality, P2/P10 value is within the scope of 1.50-2.0, and second-rate
In kadsura longepedunculata raw medicinal herbs, P2/P10 value is not in this range, or is more than or less than, and deviation is larger.Therefore, it is considered that the index
It can judge kadsura longepedunculata raw medicinal herbs quality.
The quality evaluation of kadsura longepedunculata in 4 Chinese patent drug containing kadsura longepedunculata of embodiment
U.S.'s ThermoFinnigan Trace gas chromatograph；Japanese Frontier PY-3030D double click type longitudinal type is micro-
Type furnace cracker.
Gas phase condition are as follows:
Chromatographic column be UA-5 metal capillary column (30m × 0.25mmi.d. × 0.25 μm, 5% methyl polysiloxane of film thickness,
Japan) column temperature rise program be 50 DEG C of initial temperature, be raised to 200 DEG C with 10 DEG C/min rate, then be raised to 300 with 10 DEG C/min rate
DEG C, keep 10min；Injector temperature is 300 DEG C, and detector temperature is 300 DEG C, split ratio 30:1；Carrier gas be nitrogen or helium,
Flow velocity 1.0mL/min.
Cracker condition: cracking furnace temperature: 300 DEG C；300 DEG C of vapor-phase thermal cracking device interface temperature.
Chinese patent drug containing kadsura longepedunculata is analyzed, evaluation wherein kadsura longepedunculata quality is attempted.Sample list is shown in Table
5.
Table 5: the commercially available Chinese patent drug list containing kadsura longepedunculata
The Chinese patent drug of based on kadsura longepedunculata (C-1 to C-6) is measured first.For C-1 sample, capsule is peeled off, it is taken out
Middle powder, and precise；For C-2 and C-3 sample, capsule is peeled off, takes out wherein liquid solution, precise；For
Sample C-4 to C-6 sample, directly weighing and ground 120 mesh, for use.The loading of about 0.3mg sample is accurately weighed when use
Specimen cup after being fixed on sample feeding rod, is packed into the cracker being mounted on above GC injection port, sample is in room temperature at this time.Wait crack
When device temperature reaches 300 DEG C, sample introduction button is pressed, specimen cup falls into the furnace heart, and volatile component transient evaporation brings GC by carrier gas
Injection port is analyzed.
Fig. 3 is the Flash evaporation gas chromatography figure of the main Chinese patent drug containing kadsura longepedunculata of C-1 to C-6 this 6,12 lignanoids
Quantitative result be shown in Table 6.From in figure and table in it can be seen that 6 samples in 12 lignanoids can be seen substantially, pacify five rouge
Plain (No. 1 peak), schizandrin A (No. 2 peaks) and Schisantherin C (No. 10 peaks) remain the highest lignans of content.Meter
The value for calculating 6 sample P 2/P10, the results are shown in Table 6.As can be known from Table 6, in 6 Chinese patent drug samples P2/P10 value in 1.57-
Between 1.93, the preferable standard of 1.50-2.0 mass before meeting, therefore, it is considered that kadsura longepedunculata quality used in 6 Chinese patent drugs compared with
It is good.
In addition it is noted that each Chinese patent drug is labelled with the content or hammer butt of a kind of lignanoid in 6 Chinese patent drugs
Rouge cellulose content.The quantitative result of this method is shown in Table 7 with its sign value.The result shows that the measurement result and mark of this method
It is worth close, illustrates credible result.
Then the lignanoid in the Chinese patent drug supplemented by kadsura longepedunculata is measured, to judge the quality of wherein kadsura longepedunculata.
Fig. 4 is the Flash evaporation gas chromatography figure of totally 7 Chinese patent drugs supplemented by kadsura longepedunculata of C-7 to 13.It can be seen from the figure that due to
As auxiliary material, therefore wherein, not all lignanoid can observe kadsura longepedunculata, but anwulignan (No. 1 peak), Schisandra chinensis first
Plain (No. 2 peaks) and Schisantherin C (No. 10 peaks) are still the highest lignanoid of content.Schizandrin A and Schisantherin C
Content and the content of the two substances ratio (P2/P10) are listed in Table 8 below.As shown in Table 8, P2/P10 value exists in this 7 Chinese patent drugs
Between 1.55-1.76, the range of 1.5-2.0 before meeting, therefore, it is considered that in 7 Chinese patent drugs contained kadsura longepedunculata quality compared with
It is good.
Lignanoid's content (mg/g) in 8:7, the table Chinese patent drugs supplemented by kadsura longepedunculata
Mark-on reclaims are carried out to two Chinese patent drugs of C-1 and C-10.0.5,1.0 and 1.5 times of measured amount is added, calculates its mark-on
The rate of recovery.It the results are shown in Table 9.The result shows that this method recovery of standard addition is between 90.0-106.7, RSD is less than 5.62%.
Claims (7)
1. a kind of method that flash distillation gas chromatography evaluates kadsura longepedunculata quality in commercially available Chinese patent drug, the method are as follows:
(1) the powdered or liquid Chinese patent drug sample containing kadsura longepedunculata is fitted into cracker, cracker is placed in gas phase
At injection port of chromatograph, the sample introduction when cracker temperature reaches certain temperature is detected with gas chromatograph, obtains gas-chromatography
Figure carries out qualitative analysis using the lignans in standard substance retention time centering analysing pharmaceutical samples, determines gas chromatogram
Middle anwulignan, schizandrin A and the corresponding peak position of Schisantherin C；
(2) then pass through the schizandrin A and schisantherin in external standard method centering analysing pharmaceutical samples using Flash evaporation gas chromatography method
First carries out quantitative analysis, if quantitative result is shown, the relative amount of schizandrin A and Schisantherin C is fallen in Chinese patent drug sample
Within the scope of 1.50-2.0, then contained kadsura longepedunculata quality is preferable in Chinese patent drug sample, otherwise second-rate.
2. the method as described in claim 1, it is characterised in that: the partial size of the powdered Chinese patent drug sample containing kadsura longepedunculata is 80
~120 meshes.
3. the method as described in claim 1, it is characterised in that: in step (1), using in standard substance retention time pair at
On the basis of lignans in medicine sample carry out qualitative analysis, using the lignanoid in interpretation of mass spectra centering analysing pharmaceutical samples at
Point it is qualitative further confirmed that, Mass Spectrometry Conditions are as follows: electron impact ion source, 230~250 DEG C of ion source temperature, transmission line
250~300 DEG C of temperature, ionizing energy 70eV, 50~650m/z of ion scan range.
4. the method as described in claim 1, it is characterised in that: in step (2), by external standard method to five in lignans
Taste A prime and Schisantherin C carry out quantitative analysis, are to be made into the standard items of schizandrin A and Schisantherin C first
Then the methanol solution of 20-10000mg/L is surveyed under the conditions of gas-chromatography same as Chinese patent drug sample and cracker
It is fixed, and standard curve is made in test result, the schizandrin A and five in Chinese patent drug sample is calculated according to standard curve
The content of taste ester first.
5. the method as described in one of Claims 1 to 4, it is characterised in that: carried out using Flash evaporation gas chromatography method qualitative and fixed
Measure the condition of analysis are as follows:
The GC conditions are as follows: chromatographic column is low-pole column, and column temperature rise program is 50 DEG C of initial temperature, with 5~10 DEG C/min
Rate is raised to 200 DEG C, then is raised to 300 DEG C with 3~5 DEG C/min rate, then in 300 DEG C of 5~15min of holding；Injector temperature
It is 280~320 DEG C, detector temperature is 280~320 DEG C, 30~50:1 of split ratio；Carrier gas is nitrogen or helium, flow velocity
1.0mL/min；
Cracker condition: cracking furnace temperature: 300-350 DEG C；Cracker with 300~350 DEG C of gas chromatograph interface temperature.
6. method as claimed in claim 5, it is characterised in that: the chromatographic column is UA-5 metal capillary column.
7. method as claimed in claim 6, it is characterised in that: the GC conditions are as follows: column temperature rise program is initial temperature
50 DEG C, 200 DEG C are raised to 10 DEG C/min rate, then be raised to 300 DEG C with 5 DEG C/min rate, then in 300 DEG C of holding 10min；Into
Sample mouth temperature is 300 DEG C, and detector temperature is 300 DEG C.
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